CN108039283B - A kind of rich N doping multi-stage porous carbon material and the preparation method and application thereof based on in-situ polymerization - Google Patents
A kind of rich N doping multi-stage porous carbon material and the preparation method and application thereof based on in-situ polymerization Download PDFInfo
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Abstract
The invention discloses a kind of rich N doping multi-stage porous carbon material and the preparation method and application thereof based on in-situ polymerization, it is prepared as follows to obtain: imdazole derivatives and hexachlorobutadiene is mixed, ultrasonic 1h, confined reaction 4h~12h under conditions of temperature is 180~220 DEG C, pressure release later is normal pressure, drying, obtains solid matter；Under the protection of inert gas, by obtained solid substance in 700~900 DEG C of progress high-temperature process to get finished product；Rich N doping multi-stage porous carbon material provided by the present invention based on in-situ polymerization, with excellent chemical property, it can be used to prepare electrode for capacitors especially electrode of super capacitor, so as to for there is great application potential and industrial value in energy storage field in capacitor especially supercapacitor.
Description
Technical field
The present invention provides a kind of rich N doping multi-stage porous carbon material of in-situ polymerization that can be used for supercapacitor and its
Preparation method and purposes, belong to inorganic functional material field.
Background technique
Supercapacitor is a kind of power-type energy storage device, and the ability with fast charging and discharging is used as hybrid electric
Automobile power equipment has broad application prospects.The performance of capacitor and the characteristic of electrode material have close ties.Usually
In the case of, electrode material needs that specific surface area is high, pore-size distribution is suitable for, excellent electric conductivity, physical and chemical stability are high, corrosion-resistant
Property the characteristics such as high and cheap and easy to get.
Carbon material is widely used because of large specific surface area, light weight, stability height.But carbon material as electrode material also
It is low that there are energy densities, it is therefore desirable to is further modified to carbon material.Such as other elements are adulterated in carbon material surface
(nitrogen, oxygen, phosphorus, sulphur) etc., can effectively improve the energy density of supercapacitor.Currently, nitrogen doped improve material property into
And its capacitive property is improved as the focus of attention.
Nitrating carbon material is applied to supercapacitor and mainly carries out energy storage in two ways.One is with electric double layer capacitance
Form carries out energy storage, and another kind is the progress energy storage in the form of fake capacitance.Wherein, electric double layer capacitance results from charge in electrode material
Material and the accumulation at electrolyte interface, and fake capacitance is to carry out Rapid reversible oxidation in the electrolytic solution using active material in electrode
Reduction reaction generates charge.Nitrogen material local environment is different in nitrating carbon material, can cause different chemical properties.Study table
Bright, pyrroles's nitrogen and pyridine nitrogen can effectively contribute Faraday pseudo-capacitance, both nitrogen-containing functional groups can mention to a certain extent
The hydrophily of high material, so that electrolyte is in close contact on electrode material.Graphitization nitrogen is usually located at the center of carbon net,
The electric conductivity that material can effectively be improved can quickly carry out electronics transfer in carbon material, and then reduce the charge of material
Transfer resistance obtains advantageous capacitor stability and higher high rate performance.Introducing of the nitrogen-doped carbon material due to fake capacitance
Electrode material is set to obtain biggish capacitance, while capacitive property is greatly improved, and nitrating carbon material is used for electrode material
Material will have good application prospect.
As the prior art of synthesis N doping multi-stage porous carbon material, such as can be listed below:
CN101450799 discloses a kind of graphite arc discharge method for preparing nitrogen doped carbon nanotube, nitrogen doped carbon nanotube
And the carbon nanotube original part using it.In the arc discharge method for preparing nitrogen doped carbon nanotube, using include graphite, urge
The mixture of agent and the itrogenous organic substance as nitrogen source prepares anode, and using the anode and cathode carry out arc discharge with
Prepare the nitrogen doped carbon nanotube.But the method needs higher equipment requirement, it is difficult to industrialize.
CN104934237A discloses a kind of preparation method of nitrating porous charcoal/graphene two dimension combination electrode material,
Steps are as follows: (1) graphene oxide ultrasonic disperse being obtained in solvent suspension, organic monomer is added, mechanical stirring mixes
Afterwards, initiator initiated polymerization is added, after the reaction was completed through suction filtration, wash, be dried to obtain polymer/graphene oxide two-dimensional
Composite material；(2) product and potassium hydroxide that step (1) obtains are passed through dry mixed in proportion to be placed in tube furnace,
High-temperature activation is carried out under nitrogen protection, activation products obtain target product after acid elution, deionized water washing, drying.The hair
Bright composite material obtained is two-dimensional structure, and material electric conductivity is good, but reaction process is complicated, needs potassium hydroxide living
Change, post-processing difficulty etc..
CN106887340A discloses a kind of nitrating porous carbon materials based on cytimidine, by cytimidine, resorcinol and
Formaldehyde synthesizes Nitrogen-containing Phenolic Resins by hydro-thermal method, is then freeze-dried, then after uniformly mixing activated processing with alkali, carries out
Washing is dried and is obtained, and specific surface area range is in 1700~2900m2g-1, it is 297 as its specific capacitance of capacitor electrode material
~392F/g.Although the material for the high-specific surface area that the method obtains, the content of N doping is lower, and energy density is not
It is high.
As described above, disclosing a variety of methods for preparing N doping new material using technology in the prior art, and thus
A variety of new materials with excellent electrical properties are obtained, although these N doping new materials have preferably than electricity
Hold, stability, but there are still high current charge-discharges in performance it is poor, energy density is lower the defects of, while in technique, react
Process is complicated, requirement to equipment is high, this severely limits its actual application and industrialized productions.
Therefore, how based on the defect for preparing high content nitrogen doping carbon material at present, its performance is improved using new method and had
It is of great significance, and the research hotspot and emphasis of electrochemical energy source domain at present, and this is also exactly that the present invention is able to
Where the basis of completion and where power.
Summary of the invention
The present invention overcome the problems, such as it is of the existing technology, and provide the rich N doping multi-stage porous carbon material based on in-situ polymerization
And the preparation method and application thereof.
It realizes the first aspect of the invention, provides rich N doping multi-stage porous carbon material and its preparation of in-situ polymerization
Method, the technical scheme comprises the following steps:
(1) it using imdazole derivatives and hexachlorobutadiene as raw material, is carried out under the reaction pressure for being higher than standard atmospheric pressure close
Home position polymerization reaction is closed, solid matter is obtained,
(2) solid matter is subjected under protective atmosphere the high temperature anneal, obtains rich N doping multi-stage porous carbon material.
It is 2- 5-nitro imidazole, 1,1- thio-carbonyldiimidazole, 2- that further setting, which is the imdazole derivatives,
Sulfydryl -1- methylimidazole, N, any one of N '-carbonyl dimidazoles, carbendazim, L-Histidine, Dimetridazole, imidazoles.
Further setting is that reaction pressure is 1~10MPa, reaction temperature is 180~220 DEG C in the step (1), closed
The reaction time of reaction in-situ is 4h~12h.
It is 700~1000 DEG C that further setting, which is the temperature of the step (2) high temperature annealing,.
It is 2-6h that further setting, which is the time of the high temperature anneal in the step (2),.
It is inert gas that further setting, which is the protective atmosphere in the step (2),.
It is 1:(2-6 that further setting, which is the imdazole derivatives and hexachlorobutadiene by the ratio of the amount of substance).
The second aspect of the invention provides a kind of rich N doping multi-stage porous carbon material obtained such as the method.
The third aspect of the invention provides a kind of electrode for capacitors, which includes the rich nitrogen
Adulterate multi-stage porous carbon material.
The fourth aspect of the invention provides a kind of electrode for capacitors preparation method, and technical solution is will be described
Rich N doping multi-stage porous carbon material, acetylene black and PTFE emulsion are uniformly mixed, and are coated onto nickel foam after stirring to starchiness, are coated
Amount is 1~5mg/cm2, then coated nickel foam is dried, is dried, tabletting is to get electrode for capacitors.
It is 8:1:1 that further setting, which is the mass ratio of the rich N doping multi-stage porous carbon material, acetylene black and PTFE emulsion,.
The rich N doping multi-stage porous carbon material of the in-situ polymerization of the invention has excellent electric property, can be applied to
Capacitor area, especially supercapacitor field, have a good application prospect and industrialization potential.Specifically, of the invention
The rich N doping multi-stage porous carbon material can be applied to prepare electrode for capacitors.
The PTFE emulsion is electrode preparation field commonly known raw material, can be commercially-available by multiple channel.
Coated good nickel foam is dried, dries, the operation of tabletting also belongs to the conventional skill in capacitor area
Art means, therefore no longer repeat one by one.
Electrode for capacitors using a kind of rich nitrogen-doped porous carbon material preparation of in-situ polymerization of the present invention has
Good chemical property, such as large capacity, high power, long-life, low in cost etc. are led so as to be applied to supercapacitor
Domain.
The beneficial effects of the present invention are: the rich nitrogen-doped porous carbon material of in-situ polymerization provided by the present invention, in acid
Property electrolyte solution in, have brilliant capacitive property (highest specific capacitance reaches 684F/g, and energy density is up to 189.2Wh/kg,
Power density is up to 52.9kW/kg), good cycling stability when circle (24000 capacity retention 97.5%), the in-situ polymerization
Rich nitrogen-doped porous carbon material have excellent electric property, can be used to prepare electrode for capacitors especially super capacitor electrode
Pole, so as to for there is huge application potential and industrial value in energy storage field in supercapacitor.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
Some embodiments of invention, for those of ordinary skill in the art, without any creative labor, according to
These attached drawings obtain other attached drawings and still fall within scope of the invention.
Fig. 1 is the scanning electron microscope (SEM) photograph of the rich N doping multi-stage porous carbon material of in-situ polymerization obtained by the embodiment of the present invention 1
(SEM)；
Fig. 2 is the XRD diagram of the rich N doping multi-stage porous carbon material of the in-situ polymerization of the embodiment of the present invention 1；
Fig. 3 is the nitrogen adsorption desorption curve graph of the rich N doping multi-stage porous carbon material of the in-situ polymerization of the embodiment of the present invention 1
And graph of pore diameter distribution；
Fig. 4 is the Raman figure of the rich N doping multi-stage porous carbon material of the in-situ polymerization of the embodiment of the present invention 1；
Fig. 5 is the XPS figure of the rich N doping multi-stage porous carbon material of the in-situ polymerization of the embodiment of the present invention 1；
Fig. 6 is the XPS of the nitrogen 1s electronics of the rich N doping multi-stage porous carbon material of the in-situ polymerization of the embodiment of the present invention 1
High resolution scanning figure；
Fig. 7 is capacitor prepared by rich N doping multi-stage porous carbon material using the in-situ polymerization of the embodiment of the present invention 1
H of the electrode in 0.5M2SO4Cyclic voltammetry curve figure under different scanning rates in electrolyte；
Fig. 8 is super electricity prepared by rich N doping multi-stage porous carbon material using the in-situ polymerization of the embodiment of the present invention 1
H of the container electrode in 0.5M2SO4The constant current charge-discharge curve graph under different current densities in electrolyte；
Fig. 9 is H of the electrode of super capacitor made from C2~C3 using the embodiment of the present invention 2~3 in 0.5M2SO4Electrolysis
Cyclic voltammetry curve figure in liquid, when sweep speed is 100mV/s；
Figure 10 is H of the electrode of super capacitor made from C4~C7 using the embodiment of the present invention 4~7 in 0.5M2SO4Electricity
It solves in liquid, cyclic voltammetry curve figure when sweep speed is 100mV/s；
Figure 11 is H of the electrode of super capacitor made from C8~C11 using the embodiment of the present invention 8~11 in 0.5M2SO4
Cyclic voltammetry curve figure in electrolyte, when sweep speed is 100mV/s；
Figure 12 is electrode of super capacitor made from C12~C13 using the embodiment of the present invention 12~13 0.5M's
H2SO4Cyclic voltammetry curve figure in electrolyte, when sweep speed is 100mV/s；
Figure 13 is electrode of super capacitor made from C14~C20 using the embodiment of the present invention 14~20 0.5M's
H2SO4Constant current charge-discharge curve graph in electrolyte, when sweep speed is 1A/g；
Figure 14 is super electricity prepared by rich N doping multi-stage porous carbon material using the in-situ polymerization of the embodiment of the present invention 1
H of the container electrode in 0.5M2SO4Stable circulation figure when electrolyte；
Figure 15 is super electricity prepared by rich N doping multi-stage porous carbon material using the in-situ polymerization of the embodiment of the present invention 1
The Ragone of container electrode schemes.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, the present invention is made into one below in conjunction with attached drawing
Step ground detailed description.
Embodiment 1
(1) the 2- 5-nitro imidazole of 4.09g and 20mL hexachlorobutadiene are mixed, after ultrasonic 1h, temperature is
Confined reaction 6h under conditions of 200 DEG C, later pressure release are normal pressure, and drying obtains solid matter；
(2) under the protection of inert nitrogen gas, by step (1) obtained solid substance in 800 DEG C of progress high-temperature process 2h,
Up to the rich N doping multi-stage porous carbon material based on in-situ polymerization, it is named as C1.
Embodiment 2~3: the investigation of the reaction temperature in step (1)
In addition to the reaction temperature in step (1) is replaced with 180 DEG C and 220 DEG C respectively, other operations are constant, thus suitable
It is secondary to be carried out example 2~3, it is respectively designated as C2~C3.
Embodiment 4~7: the investigation of the amount of 2- 5-nitro imidazole is added in step (1)
Except the ratio between 2- 5-nitro imidazole and the amount of substance of hexachlorobutadiene in step (1) are replaced with 1:2,1:
3, outside 1:5,1:6, other operations are constant, thus repetitive operation embodiment 1, so that example 4~7 is sequentially carried out, by institute
It obtains composite material and is successively named as C4~C7.
Embodiment 8~11: the investigation in the reaction time in step (1)
In addition to the reaction time in step (1) is replaced with 4h, 8h, 10h, 12h respectively, other operations are constant, thus
It is sequentially carried out example 8~11, is respectively designated as C8~C11.
Embodiment 12~13: the investigation of the high-temperature process temperature in step (2)
In addition to the high-temperature process temperature in step (2) is replaced with 700 DEG C and 900 DEG C respectively, other operations are constant, from
And it is sequentially carried out example 12~13, it is respectively designated as C12~C13.
Embodiment 14~20: the investigation of different imdazole derivatives in step (1)
Except the 2- 5-nitro imidazole in step (2) is replaced with 1,1- thio-carbonyldiimidazole, 2- sulfydryl-respectively
1- methylimidazole, N, N'- carbonyl dimidazoles, carbendazim, L-Histidine, Dimetridazole, outside imidazoles, other operations are constant,
To sequentially be carried out example 14~20, it is respectively designated as C14~C20.
Embodiment 21: the preparation of electrode for capacitors
Weigh rich N doping multi-stage porous carbon material, the acetylene black, PTFE (polytetrafluoroethyl-ne of the in-situ polymerization of the preparation of embodiment 1
Alkene lotion) (three's mass ratio is 80:10:10), it is uniformly mixed, when being stirred continuously into starchiness, with 2mg/cm2Coated weight apply
To on nickel foam (1 × 1cm of size), then coated nickel foam is dried, is dried, tabletting is to get to the capacitor
Electrode.
Below to the rich N doping multi-stage porous carbon material and electrode for capacitors of in-situ polymerization made from the embodiment of the present invention
Carry out performance characterization.
(1) the rich N doping multi-stage porous carbon material of in-situ polymerization made from embodiment 1 has carried out the micro- of multiple and different means
Characterization is seen, as a result as follows:
Fig. 1 is the scanning electron microscope (SEM) photograph (SEM) of the rich N doping multi-stage porous carbon material of in-situ polymerization made from embodiment 1, from
SEM figure is it can be seen that the material is three-dimensional multistage structure carbon material；
From the XRD spectrum of Fig. 2, as seen from the figure, it is two broad characteristic peaks occur at 26 ° and 43 ° in 2 θ, is stone
Black (002) and (100) crystal face shows that prepared nitrating carbon material is the characteristic of agraphitic carbon；
It can be seen that material from the BET of Fig. 3 figure as hierarchical porous structure, and predominantly mesoporous and micropore.
The Raman figure of Fig. 4 is as can be seen that material has apparent carbon peak.
The XPS figure of Fig. 5 is as can be seen that contain carbon, nitrogen, oxygen and chlorine member in the rich N doping multi-stage porous carbon material of in-situ polymerization
Element, its further content is respectively carbon 83.8%, nitrogen 12.8%, oxygen 3.34%.Hetero atom passes through the method adulterated in situ and mixes
Nitrogen and oxygen element, heteroatomic addition are conducive to the wettability for improving carbon material and electrolyte and enhancing fake capacitance, to increase
It is powered on capacitance.
Fig. 6 is the XPS fine scanning figure of institute's Nitrogen element 1s electronics in the material, and as seen from the figure, nitrogen is mainly with pyrrole
The form of pyridine nitrogen and pyrroles's nitrogen exists.
(2) electrochemical property test
Fig. 7 is cyclic voltammogram of the electrode for capacitors made from embodiment 1 under different scanning rates.
In Fig. 7, the speed of top-down each closed curve (i.e. the highest of left half lights downward arrangement) from left side
Rate is 1mV/s, 5mV/s, 10mV/s, 50mV/s, 100mV/s, 200mV/s.From this figure, it can be seen that the material is in 100mV/s
Rate under still have preferable figure.Calculating the capacity in 1mV/s by formula is 414F/g.
Constant current charge-discharge figure of the electrode for capacitors made from embodiment 1 under different current densities when Fig. 8.
In Fig. 8, in left hand view, from a left side, right current density is successively 0.5A/g, 1A/g, 2A/g, 4A/g, 5A/g；
In right part of flg, from a left side, right current density is followed successively by 10A/g, 20A/g, 40A/g, 80A/g.From constant current charge-discharge figure
It will be seen that the material is computed capacitor and remains as 684F/g, 10A/g's in the current density charge and discharge of 0.5A/g
Current density charge and discharge are computed capacitor and remain as 385F/g, thus demonstrate the material can under low current density,
Have brilliant chemical property, surmounted it has been reported that material.Meanwhile, it is capable to which the charge and discharge under high current density, show
Excellent charge-discharge performance.
Figure 15 is electrode for capacitors prepared by rich N doping multi-stage porous carbon material using in-situ polymerization in different electric currents
Ragone figure under density.From this figure, it can be seen that under the current density (the top five-pointed star) of 0.5A/g, the energy of the material
Metric density is 189.2Wh/kg.Under the current density (rightmost side five-pointed star) of 80A/g, power density can reach 52.9kW/
kg.With it has been reported that N doping carbon material compared with, have higher energy density and power density.
By above-mentioned Fig. 4-6 as it can be seen that the rich N doping multi-stage porous carbon material of the obtained in-situ polymerization of the method for the present invention has
Excellent chemical property thus can be used as the electrode material of capacitor especially supercapacitor, have in electrochemical field
Good application prospect and industrial production potential.
(3) microscopic sdIBM-2+2q.p.approach of composite material obtained by other embodiments
A, the characterization of C2~C3 is found, micromorphology height is similar to C1, and chemical property is lower than C1, and following table is not
With the capacitance for matching lower 1A/g, it is optimal for thus demonstrating 200 DEG C of reaction temperature that C1 is taken.
B, the characterization of C4~C7 is found, micromorphology height is similar to C1, and chemical property is lower than C1, and following table is not
With the capacitance for matching lower 1A/g, the substance of 2- 5-nitro imidazole and hexachlorobutadiene that C1 is taken thus is demonstrated
The ratio between amount 1:4 be optimal.
C, the characterization of C8~C11 is found, its micromorphology height of real C8~C11 is similar to C1, and chemical property is lower than
C1, following table are the capacitance of 1A/g under the reaction time, and it is optimal for thus demonstrating the reaction time 6h that C1 is taken.
D, the characterization of C12~C13 is found, its micromorphology height of C12~C13 is similar to C1, and chemical property is lower than
C1, following table are the capacitance of 1A/g at a temperature of different high-temperature process, thus demonstrate 800 DEG C of high-temperature process temperature that C1 is taken
When to be optimal.
E, the characterization of C14~C20 is found, chemical property is lower than C1, and following table is under different imdazole derivatives 1A/g
Capacitance, it is optimal for thus demonstrating the 2- 5-nitro imidazole that C1 is taken.
In conclusion the present invention passes through the selection of suitable reactants and condition, and synthesizes and obtained the rich nitrogen of in-situ polymerization
Multi-stage porous carbon material is adulterated, by the way that the study found that the composite material has excellent chemical property, there is good industry
Change application potential and market value.
It should be appreciated that the purposes of these embodiments is merely to illustrate the present invention and is not intended to limit protection model of the invention
It encloses.In addition, it should also be understood that, after reading the technical contents of the present invention, those skilled in the art can make the present invention each
Kind change, modification and/or modification, all these equivalent forms equally fall within guarantor defined by the application the appended claims
Within the scope of shield.
Claims (4)
1. a kind of preparation method of the rich N doping multi-stage porous carbon material based on in-situ polymerization, it is characterised in that including following step
It is rapid:
(1) using imdazole derivatives and hexachlorobutadiene as raw material, closed original is carried out under the reaction pressure for being higher than standard atmospheric pressure
Position polymerization reaction, obtains solid matter；
(2) solid matter is subjected under protective atmosphere the high temperature anneal, obtains rich N doping multi-stage porous carbon material；
The imdazole derivatives are 2- 5-nitro imidazole；
Reaction pressure is 1~10MPa in the step (1), reaction temperature is 180~220 DEG C, when the reaction of closed reaction in-situ
Between be 4h~12h；
The temperature of step (2) the high temperature annealing is 700~900 DEG C；
The time of the high temperature anneal in the step (2) is 2~6h；
Protective atmosphere in the step (2) is inert gas；
The imdazole derivatives and hexachlorobutadiene are 1:(2-6 by the ratio of the amount of substance).
2. the rich N doping multi-stage porous carbon material that a kind of method as described in claim 1 obtains.
3. a kind of electrode for capacitors, it is characterised in that: the electrode for capacitors includes that rich N doping as claimed in claim 2 is multistage
Hole carbon material.
4. a kind of preparation method of electrode for capacitors, it is characterised in that: by rich N doping multi-stage porous carbon materials as claimed in claim 2
Material, acetylene black and PTFE emulsion are uniformly mixed, and are coated onto nickel foam after stirring to starchiness, and coated weight is 1~3mg/cm2, then
Coated nickel foam is dried, is dried, tabletting is to get electrode for capacitors.
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